Pyridine → 1-Chloroethyl 2,3-dihydro-2,2-dimethyl-7-benzofuranyl carbonate

HRID 4428

반응식

HRID 4428 반응식
[Cl:1][CH:2]([O:4][C:5](Cl)=[O:6])[CH3:3].[CH3:8][C:9]1([CH3:19])[CH2:13][C:12]2[CH:14]=[CH:15][CH:16]=[C:17]([OH:18])[C:11]=2[O:10]1.N1C=CC=CC=1>ClCCl>[C:5](=[O:6])([O:18][C:17]1[C:11]2[O:10][C:9]([CH3:19])([CH3:8])[CH2:13][C:12]=2[CH:14]=[CH:15][CH:16]=1)[O:4][CH:2]([Cl:1])[CH3:3]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 152782,3-Dihydro-2,2-dimethyl-7-benzofuranolHCID 5213051-Chloroethyl chloroformate

생성물 1

HCID 135570951-Chloroethyl 2,3-dihydro-2,2-dimethyl-7-benzofuranyl carbonate수율 84%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
20 °C

실험 절차

21.5 g (0.15 mole) of 1-chloroethylchloroformate are added in a single portion to a solution of 2,3-dihydro-2,2-dimethyl-7-benzofuranol (24.6 g; 0.15 mole) in dichloromethane (150 ml). The mixture is cooled to between 0° and 5° C., and 12 g (0.15 mole) of pyridine are added dropwise. The mixture is stirred for 3 hours at 20° C. The organic phase is then washed with 2×50 ml of iced water. It is dried over magnesium sulphate and the solvent is evaporated. A yellow oil is obtained which is distilled. 34.1 g of the expected carbonate is then recovered (84% yield).

후처리

  1. temperatureThe mixture is cooled to between 0° and 5° C.
  2. washThe organic phase is then washed with 2×50 ml of iced water
  3. dry with materialIt is dried over magnesium sulphate
  4. customthe solvent is evaporated
  5. customA yellow oil is obtained which
  6. distillationis distilled
  7. custom34.1 g of the expected carbonate is then recovered (84% yield)

출처 및 근거

ORD 기록
ord-3c480d95de8546edb218b0eba0488c82
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725680

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